EP0971046B1 - Procede servant a fabriquer un element de revetement par pulverisation d'alliage a fusion automatique - Google Patents

Procede servant a fabriquer un element de revetement par pulverisation d'alliage a fusion automatique Download PDF

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Publication number
EP0971046B1
EP0971046B1 EP99900159A EP99900159A EP0971046B1 EP 0971046 B1 EP0971046 B1 EP 0971046B1 EP 99900159 A EP99900159 A EP 99900159A EP 99900159 A EP99900159 A EP 99900159A EP 0971046 B1 EP0971046 B1 EP 0971046B1
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EP
European Patent Office
Prior art keywords
self
sprayed coating
coating
fluxing alloy
heating
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EP99900159A
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German (de)
English (en)
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EP0971046A4 (fr
EP0971046A1 (fr
Inventor
Yoshio Harada
Hidetoshi Shin
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Tocalo Co Ltd
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Tocalo Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/18—After-treatment

Definitions

  • This invention relates to a method of producing a self-fluxing alloy spray-coated member and more particularly it proposes a novel refusing treatment method for forming a strong self-fluxing alloy sprayed coating on a surface of a substrate.
  • the technique used in the invention is a technique wherein the self-fluxing alloy sprayed coating is refused by heating to not lower than its melting point to promote densification of such a coating and metallurgical bond to the substrate (alloy layer). And also, such a technique is applicable to the other metal and alloy.
  • the spraying method is a surface treatment method wherein fine powder of metal, ceramic, cermet or the like is fused by using plasma or a combustion energy of a combustible gas and sprayed onto a surface of a substrate to from a sprayed coating.
  • metal powder when metal powder is sprayed in air, fine metal particles of fused state contact with air to produce an oxide film on the surface of the particle.
  • a metal sprayed coating has a particle lamination structure of piling fine metal particles having a thin oxide film on their surfaces one upon the other. Therefore, the sprayed coating has problems that bonding force between mutual laminated metal particles constituting the coating is weak and the coating becomes porous to bring about the lowering of the adhesion property to the metal substrate.
  • the material for the above self-fluxing alloy spraying is a low melting point material consisting essentially of Ni or Co and added with C, Cr, Fe,, Mo, Cu, W or the like and further added with Si (1.5 ⁇ 5.0 wt%) and B (1.0 ⁇ 4.5 wt%).
  • This material lies in a point that the formation of oxide on the sprayed coating is prevented and hard chromium carbide and metal boride are formed to improve the wear resistance.
  • it is said that as the above material it is favorable to use a spraying material of cermet state obtained by mixing the self-fluxing alloy and WC powder if it is intended to more enhance the wear resistance of the sprayed coating.
  • the conventional techniques for the self-fluxing alloy sprayed coating are researches and development on not only the improvement of coating properties and enlargement of their application field but also the heating and fusing treatment of the coating, but they are not yet completed to sufficient level and have the following technical problems at the present time.
  • EP-A-0185430 discloses a method for producing thick spray coated layers of a self-fluxing alloy.
  • the alloy layer is spray coated with a ceramic layer (eg a mixed oxide layer of alumina and titania).
  • An outer temperature indicating layer may be provided on top of the ceramic layer.
  • the resulting structure is then heated to fuse the alloy layer and subsequently the ceramic layer is removed.
  • the present invention seeks to propose a method capable of preventing the fusion drop-off phenomenon of the coating when the self-fluxing alloy sprayed coating is subjected to the refusing treatment.
  • the present invention also seeks to propose a method capable of preventing the ununiformization of the coating thickness due to the flowing of the coating.
  • the present invention also seeks to produce a member coated with a self-fluxing alloy sprayed coating having a smooth surface.
  • ceramics selected from oxides, nitrides, carbides and borides having a specific gravity of not more than 8.0 or a mixed ceramic of two or more thereof as a ceramic to be spray-coated on the self-flux alloy sprayed coating.
  • the self-fluxing alloy sprayed coating is heated to at least a flowing point to render into a refused state, so that air or gas (gas used in the spraying) included in the coating are efficiently discharged and also the bonding force between mutual sprayed particles constituting the coating and metallurgical bonding force to the substrate are improved. Therefore, the resulting sprayed coating is less in the closed cells, so that when it is subjected to a mechanical finishing work, there can be obtained a self-fluxing alloy sprayed coating having a smooth surface.
  • a surface of a metal substrate is degreased and subjected to a blast treatment to roughen the surface, and then self-fluxing alloy powder is sprayed onto the roughened surface of the substrate by a plasma spraying method, a flame spraying method (including a high-speed flame spraying method) or the like. Thereafter, ceramic powder is sprayed onto the resulting self-fluxing alloy sprayed coating prior to refusing treatment of the sprayed coating to form a porous ceramic sprayed coating of 3 ⁇ 50 ⁇ m in thickness (porosity: 10 ⁇ 80%).
  • an oxide, a nitride, a boride, a carbide and a mixture thereof are suitable, and particularly it is favorable to use a material having a melting point higher than that of the self-fluxing alloy, hardly reacting with components of the self-fluxing alloy and a specific gravity (not more than about 0.8) smaller than that of the self-fluxing alloy.
  • the ceramic sprayed coating does not react with the self-fluxing alloy or does not fuse, if the ceramic sprayed coating is adhered to the surface of the self-fluxing alloy, it is effective to control the fluidization of the self-fluxing alloy sprayed coating to prevent the drop-off of the coating.
  • oxide Al 2 O 3 , Cr 2 O 3 , Nb 2 O 5 , WO 3 , ZrO 2 , TiO 2 , SiO 2 boride: TiB 2 , ZrB 2 , VB 2 , NbB 2 , CrB 2 , NiB nitride: TiN, AlN, BN, Si 3 N4 carbide: TiC, B 4 C, SiC, ZrC, VC, WC, Cr 3 C 2 , NbC, TaC.
  • porous ceramic sprayed coating is formed on the surface of the self-fluxing alloy sprayed coating prior to the refusing treatment of the self-fluxing alloy sprayed coating is due to he fact that if only the self-fluxing alloy sprayed coating is directly subjected to the refusing treatment by heating in an electric furnace or by heating through a high frequency induction system without forming the ceramic sprayed coating, there is caused the following problem.
  • the self-fluxing alloy sprayed coating is gradually softened with the rise of the temperature to start fusion and fluidized by continuing the heating. If the member to be treated has a large and complicated shape, the heating becomes ununiform. As a result, a portion of a fused state (viscosity is high) is existent, while there is locally produced a portion rendered into a fluidized state (viscosity is low). In this case, the portion of the fluidized state moves toward the lower side of the member to be treated because the viscosity is low, and hence the coating thickness becomes ununiform, or in extremely cases, the above portion fluidizes to cause the drop-off.
  • ceramic particles are spray-coated on the surface of the self-fluxing alloy sprayed coating prior to the heating for refusing in order to prevent the drop-off of a part of the self-fluxing alloy sprayed coating accompanied with the aforementioned ununiform heating.
  • the ceramic particles are previously sprayed, the fluidized state of the self-fluxing alloy sprayed coating is suppressed and at the same time external air can be shielded to locally stop the fluidizing action.
  • the drop-off of the coating is not caused even when the self-fluxing alloy sprayed coating is heated to such a high temperature that it is fluidized, so that the viscosity of refused coating can be more lowered and hence it is easy to remove the discharge of air or gases existing in the coating toward exterior.
  • the oxide remaining in the coating (oxide of the self-fluxing alloy produced b spraying the self-fluxing alloy in air) is separated from the alloy and easily floats up on the surface by the flux action of Si, B included as the self-fluxing alloy component because the viscosity is low and the specific gravity of the oxide is light. This means that the oxide and the like moved to the surface can be removed when the ceramic sprayed coating is removed at the post treatment or further the polishing is conducted, which is effective to provide a member having a good surface quality.
  • the ceramic sprayed coating formed on the self-fluxing alloy sprayed coating is porous. In this case, release of air (gas) and action of separating and floating oxide are smoothly conducted and also the heating of the self-fluxing alloy sprayed coating through radiation heat is carried out in a high efficiency.
  • the ceramic sprayed coating is a porous coating having a thin thickness of about 3 ⁇ 50 ⁇ m and a porosity of 10 ⁇ 80%, preferably about 20 ⁇ 80%. It is technically difficult to obtain the coating thickness of less than 3 ⁇ m, while when it exceeds 50 ⁇ m, the effect of the invention is not developed and economical merit is not obtained. On the other hand, when the porosity is less than 10%, the action of pores is less, while when it exceeds 80%, the flowing or drop-off of the self-fluxing alloy sprayed coating rendered into the fluidized state can not be prevented.
  • the member obtained by forming the ceramic sprayed coating on the surface of the self-fluxing alloy sprayed coating is then subjected to a refusing treatment for the self-fluxing alloy sprayed coating by heating.
  • a heating method a system utilizing radiation heat in an inert gas atmosphere under a reduced pressure of 1 ⁇ 300 hPa is effective.
  • the reason why the pressure of the atmosphere is restricted to the above range is due to the fact that when the pressure is less than 1 hPa, a long time is taken and the heating effect through gas convection can not be expected, while when it exceeds 300 hPa, the effect of releasing air gas component from the fused coating is degraded.
  • the indirect heating system utilizing the radiation heat in the inert gas atmosphere does not create the oxide on the surface of the self-fluxing alloy sprayed coating of the fluidized state, so that the release of air and gases included in the coating toward exterior is easy and there can be formed a dense coating having less interior and surface defects and an excellent adhesion force.
  • the ceramic sprayed coating formed on the surface of the self-fluxing alloy sprayed coating may be formed by utilizing a material developing various colors through heating in addition to a basic color inherent to the spraying material.
  • the heating temperature, heating time, heating rate and the like for the refusing treatment can be controlled by selecting and using the ceramic to be sprayed.
  • the ceramic to be sprayed For example, when white Al 2 O 3 is sprayed, even if the self-fluxing alloy coating is somewhat over-heated, there is not caused the flowing and drop-off of the sprayed coating.
  • a black coating such as Cr 2 O 3 , TiO 2 , Al 2 O 3 -TiO 2 or the like is coated, the heating time can be shortened.
  • heating means for the refusing treatment high frequency induction heating is also effective.
  • this heating system there can be used methods widely adopted in industrial fields. For example, this method is carried out by arranging a copper coil capable of flowing a cooling water around the member to be heated and supplying a high frequency current to the coil. Moreover, current, voltage, frequency, heating time and the like required for the heating are properly selected in accordance with the size of the member to be heated.
  • the ceramic coating formed on the surface of the self-fluxing alloy sprayed coating is removed by various methods. Therefore, the ceramic sprayed coating is not necessarily required to have a good adhesion property, so that the spraying method is not particularly restricted.
  • the coating can be formed by spraying alumina powder or the like with a high pressure air, it is possible to attain the method according to the invention by the above method.
  • the self-fluxing alloy sprayed coating is refused by heating, it is cooled and the ceramic sprayed coating adhered to the surface of the alloy coating is removed by spraying powder such as mineral slug, silica sand, Al 2 O 3 or the like. Thereafter, it is subjected to cutting, polishing and further mirror finishing until the surface of the self-fluxing alloy sprayed coating is completely exposed by mechanical working, if necessary.
  • the thus obtained self-fluxing alloy sprayed coating according to the invention is less in the pores retained in its inside and small in the pore size and the oxide film produced in the spraying gathers on the surface, so that a very smooth finished surface is obtained.
  • self-fluxing alloy adapted to the method of the invention, there can be mentioned not only Ni-based, Co-based alloys defined in JIS H8303 Self-Fluxing Alloy Spraying and alloy obtained by dispersing WC particles into Co-based alloy but also Fe-based alloy (for example; 0.05C-4Si-35Cr-3.4B-remainder of Fe (wt%), melting point: 1115°C).
  • a self-fluxing alloy sprayed coating is subjected to a refusing treatment under heating by various methods and thereafter a section of the sprayed coating is observed by means of an optical microscope to measure remaining bubble and a joint state to a member to be treated.
  • Ni-based self-fluxing alloy us used as a self-fluxing alloy spraying material.
  • Table 1 also shows Ni-based alloy as an alloy B, Co-based self-fluxing alloy as an alloy C, Ni-based self-fluxing alloy containing WC particles as an alloy D, and Fe-based self-fluxing alloy as an alloy E.
  • a steel pipe having an outer diameter of 38 mm, a gauge of 3.2 mm and a length of 100 mm is used as a member to be treated.
  • a self-fluxing alloy having an apparent thickness of 0.8 mm is formed on an outer surface of the member to be treated by a flame spraying method.
  • the heating is stopped at a time that a wetting and shining phenomenon of the coating arrived at its melting point is caused by visual observation, and then the coating is cooled to room temperature and cut for the measurement through microscope.
  • the coating according to the invention (No. 1) heated under a reduced pressure of 10 hPa in N 2 gas after air is removed from the heating atmosphere, when the coating is fused, the generation of gas and release thereof are easy because of negative pressure, so that it has been found that the pores left in the coating are less and the pore diameter is smallest and the diffusion bond state to the member to be treated is even.
  • Heating method Pore distribution Pore diameter ( ⁇ m) Metallurgical bond to member to be treated Remarks 1 Heating in inert gas under a reduced pressure Evenness 1 ⁇ 5 Uniform Acceptable example 2 High frequency induction heating Relatively evenness 8 ⁇ 15 Uniform Comparative example 3 Heating by combustion flame Unevenness 10 ⁇ 50 Ununiform Comparative example (Note) (1) reduced pressure condition 10hPa N 2 (2) frequency 2KH z power 70KW (3) Combustion flame is oxygen-acetylene flame
  • a coating having a thickness of 0.7 mm is formed on the surface of the member to be treated by using the same spraying method as in Example 1.
  • the heating-fusing method of the self-fluxing alloy sprayed coating is used an electric furnace capable of controlling atmosphere, wherein air in the electric furnace is first removed by a vacuum pump (1x10-3 hPa) and then Ar gas is introduced to adjust a partial pressure to 0.1, 1, 10, 100 or 1000 hPa and thereafter temperature is raised by heating.
  • the heating temperature is 1050°C at maximum in the alloy B and 1170°C in the alloy C.
  • Fig. 1 shows a relation between outer diameter of pore and Ar partial pressure as a heating atmosphere.
  • the pore diameter retained in the coating is smaller in the alloy B than that in the alloy C, and also the pore diameter becomes small when the Ar partial pressure is within a range of 0.1 ⁇ 300 hPa.
  • the melting point is high because Co is a main component, and the viscosity is high even at the fused state, so that the release of gas components is slow.
  • the fluidity is good and the release of gas component is fast and the number of pores is small and only small pores are retained.
  • a porous Al 2 O 3 sprayed coating having a porosity of 18 ⁇ 28% is formed on the self-fluxing alloy sprayed coating at a thickness of 30 ⁇ m as a top coat.
  • the alloys B and C of No. 3 and No. 4 shown as a comparative example do not fuse at a low temperature and do not indicate the properties as a self-fluxing alloy.
  • the former alloy is fused at about 1030°C, while the latter alloy is fused at about 1150°C, whereby there is formed a dense coating including small pores.
  • both coatings are fluidized when the temperature is further raised (1055°C, 1170°C) and flow downward by their dead weight, and hence the coating thickness becomes ununiform.
  • the coating forming Al 2 O 3 as a top coat does not flow downward even at the same temperature and maintains the initial thickness.
  • the viscosity of the coating lowers, and the release of gases from exterior and reduction action of oxide by elementary Si, B included in the self-fluxing alloy are active and oxides and the like having a light specific gravity are easily floated from the surface of the coating, so that the number of pores in the inside of the coating is less and the homogeneous coating is obtained.
  • the drop-off of the self-fluxing alloy is controlled, so that it is possible to conduct a higher temperature heating as compared with the self-fluxing alloy coating having no top coat, and hence the size of the pores left in the coating is decreased and also the temperature control range is made large and the improvement of the productivity can be expected.
  • Coating structure Melting point of self-fluxing alloy (°C) Heating property of coating, fluidized drop-off temperature (°C) Pore diameter remaining on section of coating after heat fusion ( ⁇ m) Remarks Self-fluxing alloy Top coat 1 Alloy B Al 2 O 3 1030 ⁇ 5 1070 ⁇ 5 1 ⁇ 3 Acceptable example 2 Alloy C Al 2 O 3 1150 ⁇ 5 1195 ⁇ 5 0.8 ⁇ 3 3 Alloy B None 1030 ⁇ 5 1055 ⁇ 5 1 ⁇ 5 Comparative example 4 Alloy C None 1150 ⁇ 5 1170 ⁇ 5 1 ⁇ 5
  • the change of diameter in pores left inside the coating is examined when the porous ceramic sprayed layer is formed on the self-fluxing alloy sprayed coating as a top coat and treated by a high frequency induction heating system.
  • Each of the above alloys D and E is sprayed at a thickness of 1.0 mm by a plasma spraying method, while the coating according to the invention is further laminated with Al 2 O 3 having a porosity of 12-30% and a thickness of 25 ⁇ m as a top coat.
  • the self-fluxing alloy spayed coating is heated and fused by using a high frequency induction heating system (frequency: 2 kHz) and gradually moving a high frequency ring disposed at the outside of the member to be treated.
  • a high frequency induction heating system frequency: 2 kHz
  • Table 4 results examined on cut section of the self-fluxing alloy coating after the high frequency induction heating by means of an optical microscope.
  • Table 4 when the coatings of the comparative examples (No. 3, 4) are compared with those formed by the heating method of combustion flame shown in Table 2, the pores are relatively dense and small. In the coatings according to the invention, however, the flowing or drop-off of the coating is not caused even when it is maintained at a temperature higher by about 10 ⁇ 20°C than that of the above comparative example, and the pores remaining in the coating are more dense and very small.
  • the porous ceramic sprayed coating is temporarily formed prior to the refusing treatment of the self-fluxing alloy sprayed coating, so that it is possible to prevent the flowing and drop-off phenomenon of the self-fluxing alloy sprayed coating. Therefore, the higher temperature heating is possible as compared with the case of the usual self-fluxing alloy sprayed coating and hence the viscosity of the sprayed coating is lowered to promote the release of gases. Further, the floating of the oxide is easy and the surface quality of the self-fluxing alloy sprayed coating after the removal of the ceramic sprayed coating is good.
  • the rejection rate of the members covered with the self-fluxing alloy sprayed coating requiring precise finish can considerably be decreased.
  • the operation for refusing treatment of the sprayed coating is easy.
  • the members covered with the self-fluxing alloy sprayed coating produced by the method according to the invention can be used various rollers, bush, sleeve, plunger, impeller, mechanical seal protection tube, crusher hammer, piston rod, mold, pelletizer dies and capstan in fields of production of iron-steel and nonferrous materials, members in galvanization plating bath, pump and valves, petroleum purification, petrochemical apparatuses, coal transporting devices, die-cast, production apparatuses for glass products and the like.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Coating By Spraying Or Casting (AREA)

Claims (4)

  1. Procédé de production d'un élément de revêtement enduit par pulvérisation d'alliage autodécapant en appliquant un revêtement par pulvérisation d'alliage autodécapant ramolli ou refondu sur une surface d'un substrat en acier, caractérisé en ce qu'un alliage autodécapant est enduit par pulvérisation sur une surface, et un revêtement par pulvérisation de céramique ayant une porosité de 10 à 80 % et une épaisseur de 3 à 50 µm est formé sur celui-ci, puis les éléments enduits par pulvérisation obtenus sont chauffés dans une atmosphère de gaz inerte sous une pression réduite de 1 à 300 hPa pour refondre le revêtement par pulvérisation d'alliage autodécapant et ensuite, le revêtement par pulvérisation de céramique formé sur une couche externe des éléments est retiré pour exposer de nouveau le revêtement par pulvérisation d'alliage autodécapant.
  2. Procédé de production d'un élément de revêtement enduit par pulvérisation d'un alliage autodécapant en appliquant un revêtement par pulvérisation d'alliage autodécapant ramolli ou refondu sur une surface d'un substrat en acier, caractérisé en ce qu'un alliage autodécapant est enduit par pulvérisation sur une surface, et un revêtement par pulvérisation de céramique ayant une porosité de 10 à 80 % et une épaisseur de 3 à 50 µm est formé sur celui-ci, puis ces revêtements par pulvérisation sont soumis à un chauffage inductif à fréquence élevée dans une atmosphère de gaz inerte pour refondre le revêtement par pulvérisation d'alliage autodécapant et, ensuite, le revêtement par pulvérisation de céramique formé sur une couche externe des éléments est retiré pour exposer de nouveau le revêtement par pulvérisation d'alliage autodécapant.
  3. Procédé selon la revendication 1 ou 2, dans lequel l'une des céramiques choisie parmi des oxydes, des nitrures, des carbures et des borures ayant une densité non supérieure à 8,0 ou une céramique mixte de deux ou plus parmi ceux-ci est utilisée en tant que céramique à enduire par pulvérisation sur le revêtement par pulvérisation d'alliage autodécapant.
  4. Procédé selon l'une quelconque des revendications précédentes, dans lequel la vitesse d'augmentation de température et la température de chauffage sont ajustées en fonction de la couleur du revêtement par pulvérisation de céramique dans le traitement de refonte du revêtement par pulvérisation.
EP99900159A 1998-01-29 1999-01-11 Procede servant a fabriquer un element de revetement par pulverisation d'alliage a fusion automatique Expired - Lifetime EP0971046B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP01704798A JP3204637B2 (ja) 1998-01-29 1998-01-29 自溶合金溶射被覆部材の製造方法
JP1704798 1998-01-29
PCT/JP1999/000050 WO1999039020A1 (fr) 1998-01-29 1999-01-11 Procede servant a fabriquer un element de revetement par pulverisation d'alliage a fusion automatique

Publications (3)

Publication Number Publication Date
EP0971046A1 EP0971046A1 (fr) 2000-01-12
EP0971046A4 EP0971046A4 (fr) 2002-07-03
EP0971046B1 true EP0971046B1 (fr) 2004-04-14

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US (1) US6326063B1 (fr)
EP (1) EP0971046B1 (fr)
JP (1) JP3204637B2 (fr)
DE (1) DE69916373T2 (fr)
WO (1) WO1999039020A1 (fr)

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JP3204637B2 (ja) 2001-09-04
US6326063B1 (en) 2001-12-04
DE69916373T2 (de) 2004-08-12
WO1999039020A1 (fr) 1999-08-05
JPH11217664A (ja) 1999-08-10
EP0971046A4 (fr) 2002-07-03
EP0971046A1 (fr) 2000-01-12
DE69916373D1 (de) 2004-05-19

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